CN107414073B - 硫化亚锡/金纳米颗粒复合物及其制备方法和应用 - Google Patents

硫化亚锡/金纳米颗粒复合物及其制备方法和应用 Download PDF

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CN107414073B
CN107414073B CN201710680158.1A CN201710680158A CN107414073B CN 107414073 B CN107414073 B CN 107414073B CN 201710680158 A CN201710680158 A CN 201710680158A CN 107414073 B CN107414073 B CN 107414073B
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晏善成
宋海增
徐欣
王俊
吴建盛
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Nanjing Post and Telecommunication University
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Abstract

本发明公开了硫化亚锡/金纳米颗粒复合物及其制备方法和应用，制备方法是：机械剥离硫化亚锡材料，产物厚度50‑100 nm,大小几微米到十几微米，氩气气氛中退火后备用；滴加氯金酸水溶液到机械剥离的硫化亚锡表面，沉积2‑5 min,氮气吹走多余的液体，120‑150℃反应时间2‑5；反应结束后，快速取出样品，得到金纳米颗粒在硫化亚锡自取向性组装，所得金纳米颗粒尺寸几十纳米，结晶性好，在光电探测器件、生物传感等领域具有广泛重要的应用前景。

Description

硫化亚锡/金纳米颗粒复合物及其制备方法和应用
技术领域
本发明涉及的是一种硫化亚锡诱导生长金纳米颗粒的自组装方法，属于纳米材料制备领域。
背景技术
硫化亚锡是性能优良的P型半导体，在很多领域具有广泛的应用，可用作晶体管、传感器、太阳能电池、开关、电池电极等。不同于诸如石墨烯等零隙半导体的是，硫化亚锡有带隙，且为间接带隙，并且其带隙和原子层数有重要的联系，层数越薄带隙越大。也不同于过度金属二维材料如二硫化钼，硫化亚锡从块体到单层都是间接带隙。但目前硫化亚锡和金纳米颗粒的复合物制备方法还鲜有报道。
金纳米颗粒的合成一般采用溶液化学还原的方法，如用乙二醇或是硼氢化钠等作为还原剂，但是该方法不能使得金纳米颗粒在衬底材料上有序组装。因此开发一种简单有效的方法原位生长金纳米颗粒/硫化亚锡复合物就显得尤为必要。
发明内容
本发明的目的是提供硫化亚锡/金纳米颗粒复合物及其制备方法和应用，工艺简单，获得的金纳米颗粒的粒径范围是几纳米到几十纳米，结晶性好。
为了实现上述发明目的，本发明采用以下技术方案：
硫化亚锡/金纳米颗粒复合物，金纳米颗粒颗粒在硫化亚锡表面具有取向性排列，金纳米颗粒尺寸在15-25纳米。
硫化亚锡/金纳米颗粒复合物的制备方法，步骤如下：
（1）机械剥离硫化亚锡材料，产物厚度50-100 nm, 大小几微米到十几微米，氩气气氛中退火后备用。
（2）滴加氯金酸水溶液到机械剥离的硫化亚锡表面，沉积2-5 min, 氮气吹走多余的液体，置于烘箱中加热反应。
氯金酸水溶液的浓度为10%-26%，滴加量为1-3µL； 反应温度为120-150℃、反应时间2-5 min。
（3）反应结束后，快速取出样品，得到金纳米颗粒在硫化亚锡自取向组装。得到金纳米颗粒在硫化亚锡自取向组装，金纳米颗粒大约几十纳米，结晶性好，该复合物在光电探测领域应用广泛。
本发明的原理说明如下：Au3+/Au0 的还原电势大约为5.5 eV(相对于真空而言)，而硫化亚锡的导带小于5.5 eV，因此电子会从硫化亚锡转移到Au3+上，使得Au3+原位还原成Au0。
本发明具有以下优点：（1）得到的产物金纳米颗粒粒径为几纳米到几十纳米，结晶性好，稳定性高；（2）工艺简单，而且成本低廉，时间较短，环境友好；（3）该方法制备的硫化亚锡/金纳米颗粒复合物性能优越，在光电探测器件、生物传感等领域具有广泛重要的应用前景。
附图说明
图1 为实施例1机械剥离的硫化亚锡样品的光学显微镜照片，从照片中可以看出该样品大小大约几个微米，厚度魏50-100 nm。
图2 为实施例1机械剥离的硫化亚锡样品的Raman图，曲线中出现了硫化亚锡的主要拉曼峰，同时还说明机械剥离所得硫化亚锡的结晶性良好。
图3 为实施例1制备得到的硫化亚锡/金纳米颗粒复合物的扫描电镜图，可知金纳米颗粒为几纳米到几十纳米，结晶性好，稳定性高，同时颗粒在硫化亚锡表面具有一定的取向排列。
具体实施方式
以下将结合实施例和附图具体说明本申请的技术方案。
硫化亚锡样品的剥离方法，参见文献（K.S. Novoselov, et al Science, 2004,306: 666-669）。
实施例1
一种硫化亚锡诱导生长金纳米颗粒的自组装方法，步骤如下：
（1）机械剥离得到硫化亚锡，其厚度大约70 nm, 大小几微米到十几微米，氩气气氛中退火后备用；
（2）将氯金酸粉末溶解到水中，得到26%的氯金酸水溶液，滴加2 µm的氯金酸水溶液到机械剥离的硫化亚锡表面，沉积2 min, 氮气吹走多余的液体，随后烘箱中反应温度为150℃、反应时间5 min；
（3）反应结束后，快速取出样品，得到金纳米颗粒在硫化亚锡自组装，金纳米颗粒大约15-25纳米，结晶性好。
实施例2
一种硫化亚锡诱导生长金纳米颗粒的自组装方法，步骤如下：
（1）机械剥离得到硫化亚锡材料，其厚度大约85 nm, 大小几微米到十几微米，氩气气氛中退火后备用；
（2）将氯金酸粉末溶解到水中，稀释得到13%的氯金酸水溶液，滴加3 µm的氯金酸水溶液到机械剥离的硫化亚锡表面，沉积3 min, 氮气吹走多余的液体，随后烘箱中反应温度为120℃、反应时间5 min；
（3）反应结束后，快速取出样品，得到金纳米颗粒在硫化亚锡自组装，金纳米颗粒大约10-15纳米，结晶性好。
实施例3
一种硫化亚锡诱导生长金纳米颗粒的自组装方法，步骤如下：
（1）机械剥离得到硫化亚锡材料，其厚度大约100 nm, 大小几微米到十几微米，氩气气氛中退火后备用；
（2）将氯金酸粉末溶解到水中，稀释得到19%的氯金酸水溶液，滴加2 µm的氯金酸水溶液到机械剥离的硫化亚锡表面，沉积4 min, 氮气吹走多余的液体，随后烘箱中反应温度为130℃、反应时间3 min；
（3）反应结束后，快速取出样品，得到金纳米颗粒在硫化亚锡自组装，金纳米颗粒大约8-12纳米，结晶性好。
实施例4 实施例1所得复合物在光电探测领域应用案例
硫化亚锡自组装金纳米颗粒复合物可以应用于光电探测领域，将该复合物作为光电导型器件制作的材料，当光照波长和表面的金纳米颗粒耦合成表面等离子基元时，金纳米颗粒的表面电子会部分注入硫化亚锡表面，与硫化亚锡表面导电的空穴复合，抑制了光电流，因此，通过调控金纳米颗粒的大小调节和光耦合波长，就可以构建对光的波长探测器件。

Claims (1)

1.硫化亚锡/金纳米颗粒复合物的制备方法，该硫化亚锡/金纳米颗粒复合物的金纳米颗粒在硫化亚锡表面具有取向性排列，金纳米颗粒尺寸在15-25纳米，该硫化亚锡/金纳米颗粒复合物可用于光电探测领域，其特征在于，步骤如下：
（1）机械剥离硫化亚锡材料，产物厚度50-100 nm, 大小几微米到十几微米，氩气气氛中退火后备用；
（2）滴加氯金酸水溶液到机械剥离的硫化亚锡表面，沉积2-5 min, 氮气吹走多余的液体，置于烘箱中加热反应；
氯金酸水溶液的浓度为10%-26%，滴加量为1-3µL ；
反应温度为120-150℃、反应时间2-5 min；
反应结束后，快速取出样品，得到金纳米颗粒在硫化亚锡自取向组装。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101585527A (zh) * 2008-05-23 2009-11-25 中国人民解放军63971部队 一种富含中、大孔的炭材料的制备方法
WO2010048517A2 (en) * 2008-10-23 2010-04-29 Brigham Young University Data storage media containing inorganic nanomaterial data layer
CN104822477A (zh) * 2013-01-29 2015-08-05 Lg化学株式会社 用于太阳能电池的金属纳米粒子的制备方法,包含该金属纳米粒子的油墨组合物,以及使用该油墨组合物制备薄膜的方法
CN105478752A (zh) * 2015-12-14 2016-04-13 东华大学 一种微米级聚合物基复合导电金球的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101585527A (zh) * 2008-05-23 2009-11-25 中国人民解放军63971部队 一种富含中、大孔的炭材料的制备方法
WO2010048517A2 (en) * 2008-10-23 2010-04-29 Brigham Young University Data storage media containing inorganic nanomaterial data layer
CN104822477A (zh) * 2013-01-29 2015-08-05 Lg化学株式会社 用于太阳能电池的金属纳米粒子的制备方法,包含该金属纳米粒子的油墨组合物,以及使用该油墨组合物制备薄膜的方法
CN105478752A (zh) * 2015-12-14 2016-04-13 东华大学 一种微米级聚合物基复合导电金球的制备方法

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